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2-Benzylamino-7-carbethoxymethoxytetraline hydrochloride → 2-Amino-7-carbethoxymethoxytetraline hydrochloride

HRID 1590359
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HRID 1590359 반응식
[ClH:1].C([NH:9][CH:10]1[CH2:19][CH2:18][C:17]2[C:12](=[CH:13][C:14]([O:20][CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])=[CH:15][CH:16]=2)[CH2:11]1)C1C=CC=CC=1>C(O)C.O.[Pd]>[ClH:1].[NH2:9][CH:10]1[CH2:19][CH2:18][C:17]2[C:12](=[CH:13][C:14]([O:20][CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])=[CH:15][CH:16]=2)[CH2:11]1
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참가 물질

5

반응물 1

HCID 197704852-Benzylamino-7-carbethoxymethoxytetraline hydrochloride

생성물 1

HCID 200947462-Amino-7-carbethoxymethoxytetraline hydrochloride수율 92.6%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 702Ethanol용매HCID 962Water용매

실험 절차

A solution of 27 g of 2-benzylamino-7-carbethoxymethoxytetraline hydrochloride, EXAMPLE 1, in 300 ml of 95% ethanol and 25 ml of water, is hydrogenated under ordinary pressure and at temperature of 50° C. by using 3 g of 10% palladium on charcoal as a catalyst. After 3 hours, the mixture is filtered, the residue is taken up twice with 100 ml of absolte ethanol and dried every time. The product so obtained is triturated in 150 ml of acetone, filtered and crystallized from 100 ml of isopropanol to give 19 g of 2-amino-7-carbethoxymethoxytetraline hydrochloride; m.p. 143°-145° C. The product thus obtained may be used for the preparation of the compound of formula (XV) above, in which X is hydrogen and O-R' is a carbethoxymethoxy group (COMPOUND 1), as follows:

후처리

  1. customis hydrogenated under ordinary pressure and at temperature of 50° C.
  2. filtrationthe mixture is filtered
  3. customdried every time
  4. customThe product so obtained
  5. customis triturated in 150 ml of acetone
  6. filtrationfiltered
  7. customcrystallized from 100 ml of isopropanol

출처 및 근거

ORD 기록
ord-1c22c4dad87c4251a552250b0efc5486
출처 데이터셋
uspto-grants-1993_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05202466

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